关键词: 抗生素, 贝类, 超声波萃取, 固相萃取, 超高效液相色谱–三重四级杆质谱, Oasis PRiME HLB

Abstract:

A fast and simple method for simultaneous determination of fifteen antibiotics (sulfadiazine, ciprofloxacin, penicillin, spechromycin and roxithromycin) in mussels using ultrasound extraction, solid phase extraction purification and ultra performance liquid chromatography-tandem mass spectrometric was established. The mussel samples were extracted by ultrasonic extraction, followed by solid-phase extraction (SPE) as the cleanup procedure. Ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) was used for identification and quantification of antibiotics. The performance of two kinds of SPE cartridges, Oasis HLB and Oasis PRiME HLB, was compared, with the latter showing better results. Recoveries ranged from 64% to 121% at spiking levels of 50 ng/g, with RSD being 0.5%–19%, and from 67% to 117% at spiking levels of 100 ng/g, with RSD being 1%–9%. Limits of detection (LODs) ranged from 0.004 to 0.5 ng/g (dry weight) and limits of quantification (LOQs) ranged from 0.013 to 1.67 ng/g (dry weight). The recoveries were reasonable and the detection limit was low. Finally, the method was successfully applied to the determination of the target antibiotics in mussel samples (Hyriopsis cumingii) collected from Poyang Lake. 9 out of 15 selected antibiotics were detected in the collected mussel tissues. The concentration and detection frequency of trimethoprim in mussels were the highest. The concentration of trimethoprim was 78.8 ng/g, followed by spectinmycin (41.2 ng/g) and ciprofloxacin (39.8 ng/g).

Key words: antibiotics, mussels, ultrasonication extraction, solid-phase extraction, UPLC-MS/MS, Oasis PRiME HLB